CN101104139B - Method for preparing alcohol ether type surfactant polyethylene monoester phthalic acid - Google Patents
Method for preparing alcohol ether type surfactant polyethylene monoester phthalic acid Download PDFInfo
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- CN101104139B CN101104139B CN2006100523866A CN200610052386A CN101104139B CN 101104139 B CN101104139 B CN 101104139B CN 2006100523866 A CN2006100523866 A CN 2006100523866A CN 200610052386 A CN200610052386 A CN 200610052386A CN 101104139 B CN101104139 B CN 101104139B
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Abstract
The invention discloses a preparation method of the alcohol ether type surface active agent, polyethylene glycol o-benzene dicarbonic acid monoester, which takes phthalic anhydride and polyethylene glycol as materials, and the reaction duration is three to five hours under the temperature of seventy five to 75-85 DEG C with the existing of acidic catalyst, the pH value is changed to one point five-three point five after neutralization by adding alkali, the molar ratio of phthalic anhydride and polyethylene glycol is one to zero point nine-one point one. The product is characterized by wide purposes by adopting the proposal, and has outstanding effects for improving the solubility of the water-solubility dyestuff. The invention has no need for filtration, so three wastes can be avoided, thus protecting the environment; because the reaction condition is mild, the invention can be produced by the general device without safe hidden troubles. When majority of water-solubility dyestuff fully dissolves, the solution can stand still for seventy two hours without precipitation under normal temperature and maintain the homogeneous state by adding the surface active agent.
Description
Technical field
The present invention relates to the preparation method of a surfactant, the preparation method of a kind of alcohol ether type surfactant polyethylene monoester phthalic acid of more specifically saying so.
Background technology
Surfactant is a kind of compound that is not dissociated into the amphiphilic structure of ionic condition in water at surfactant.Its hydrophilic group is to be that polyoxyethylene groups one (C2H4O) n constitutes by polyethylene glycol groups, is exactly that polyalcohol (is glycerine, pentaerythrite in addition; Glucose, sorbierite etc.) be the structure on basis, also have structure in addition based on MEA, diethanol amine etc.Non-ionic surface active agent most of one-tenth liquid state or pulpous state, its aqueous solution is along with the cloud point phenomenon can appear in the rising of temperature.Because it can not be dissociated into ion in the aqueous solution, so stability is high, the influence of acid and alkali alkali salt, stability in hard water is strong, compatibility is good, can with yin, yang, the composite use of amphoteric surfactant.Non-ionic surface active agent has high surface, and the solubilising wetting action is strong, and good emulsifying power and detergency are arranged.Toxicity is low, and is less to skin irritatin, counts in the scope at certain EO, and certain biological degradability is arranged.State Intellectual Property Office is in disclosed patent documentation (publication number: CN1180075) in " a kind of preparation method of rosin acid Macrogol Ester " on April 29th, 1998, narrated its preparation method: be to be that raw material and equimolar polyethylene glycol are that catalyst carries out esterification reaction with phosphorous acid under 200～300 ℃ with rosin or disproportionation rosin, reaction time is 1-6 hours, prepare rosin acid Macrogol Ester non-ionic surface active agent. it has good reducing thick oil viscosity characteristic, but this technological reaction temperature is than higher, to the equipment potential safety hazard of having had relatively high expectations, the purposes scope is less in the building-up process.
Summary of the invention
At the problems referred to above, the problem that quasi-solution of the present invention is determined provide a kind of technology rationally, production equipment required the preparation method of lower alcohol ether type surfactant polyethylene monoester phthalic acid.
For addressing the above problem, the present invention has adopted following technical scheme: a kind of preparation method of alcohol ether type surfactant polyethylene monoester phthalic acid, it is a raw material with phthalic anhydride and polyethylene glycol, under 75～85 ℃ of temperature, reacting 3～5 hours in the presence of the acidic catalyst, add in the alkali and pH value to 1.5～3.5, the mol ratio of described phthalic anhydride and polyethylene glycol is 1: 0.9～1.1.
As preferred described reaction temperature is 78～83 ℃, and the reaction time is 3.5～4.5 hours.The preparation method of above-mentioned alcohol ether type surfactant polyethylene monoester phthalic acid, described acidic catalyst is the sulfuric acid of phosphorous acid or 98%, its consumption is 0.5～1.5% of a phthalic anhydride weight.The alkali of described neutralization is that concentration is that 30% NaOH or concentration are 30% potassium hydroxide.
Concrete reactional equation is:
Because it is active high to have adopted technique scheme, polyethylene monoester phthalic acid to have, the characteristics that purposes is wide are mainly used in fine chemistry industry and the printing and dyeing, and the solubility that improves water-soluble dye is had obvious effects.Because need not to filter,, protected environment so avoided the generation of the three wastes; Because of the reaction condition gentleness, conventional equipment can be produced, no potential safety hazard.After many water-soluble dyes are molten entirely, add this surfactant, solution is left standstill at normal temperatures keep still not separating out or keeping in 72 hours even matter state.
The specific embodiment
Embodiment 1
Get in the there-necked flask that phthalic anhydride 100 gram and 364.6 gram polyethylene glycol (PEG-600) (mol ratio is 1: 0.9) join 1000 milliliters, after mixing, the phosphorous acid catalyst that adds 0.5 gram, be warmed up to 75 ℃ and kept 5 hours, material is the water white transparency shape, add 30% potassium hydroxide again and be neutralized to pH value 3.5, promptly make about 465. gram alcohol ether type surfactant polyethylene monoester phthalic acids.
Embodiment 2
Get in the there-necked flask that phthalic anhydride 100 gram and 405.1 gram polyethylene glycol (PEG-600) (mol ratio is 1: 1) join 1000 milliliters, after mixing, the phosphorous acid catalyst that adds 1.5 grams, be warmed up to 85 ℃ and kept 3 hours, material is the water white transparency shape, add 30% NaOH again and be neutralized to pH value 1.5, promptly make about 508 gram alcohol ether type surfactant polyethylene monoester phthalic acids.
Embodiment 3
Get in the there-necked flask that phthalic anhydride 100 gram and 445.6 gram polyethylene glycol (PEG-600) (mol ratio is 1: 1.1) join 1000 milliliters, after mixing, the sulfuric acid catalyst that adds 1.0 grams 98%, be warmed up to 78 ℃ and kept 3.5 hours, material is the water white transparency shape, add 30% potassium hydroxide again and be neutralized to pH value 3.5, promptly make about 547. gram alcohol ether type surfactant polyethylene monoester phthalic acids.
Embodiment 4
(PEG-600 (mol ratio is 1: 1) joins in 1000 milliliters the there-necked flask to get phthalic anhydride 100 gram and 405.1 gram polyethylene glycol, after mixing, the sulfuric acid catalyst that adds 1.5 grams 98%, be warmed up to 83 ℃ and kept 5 hours, material is the water white transparency shape, add 30% potassium hydroxide again and be neutralized to pH value 3.0, promptly make about 508 gram alcohol ether type surfactant polyethylene monoester phthalic acids.
Embodiment 5
Get in the there-necked flask that phthalic anhydride 100 gram and 397.0 gram polyethylene glycol (PEG-600) (mol ratio is 1: 0.98) join 1000 milliliters, after mixing, the phosphorous acid catalyst that adds 1.0 grams, be warmed up to 80 ℃ and kept 2.5 hours, material is the water white transparency shape, add 30% NaOH again and be neutralized to pH value 2.5, promptly make about 498 gram alcohol ether type surfactant polyethylene monoester phthalic acids.
Applicating example: the alcohol ether type surfactant polyethylene monoester phthalic acid to the acquisition of the foregoing description 1-5 is made following application test.After the former dyestuff dry powder of adding 50 gram acid blue 5R is warmed up to 90 ℃ of whole dissolvings in 1 premium on currency, adds 2.5 and restrain o-benzenedicarboxylic acid polyethylene glycol esters, solution is left standstill at normal temperatures kept 72 hours, material still is uniform solution.
Claims (5)
1. the preparation method of an alcohol ether type surfactant polyethylene phthalic monoester, it is characterized in that it is a raw material with phthalic anhydride and polyethylene glycol, under 75～85 ℃ of temperature, reacting 3～5 hours in the presence of the acidic catalyst, add in the alkali and pH value to 1.5～3.5, the mol ratio of described phthalic anhydride and polyethylene glycol is 1: 0.9～1.1.
2. the preparation method of alcohol ether type surfactant polyethylene phthalic monoester according to claim 1 is characterized in that described reaction temperature is 78～83 ℃.
3. the preparation method of alcohol ether type surfactant polyethylene phthalic monoester according to claim 1 is characterized in that the described reaction time is 3.5～4.5 hours.
4. according to the preparation method of claim 1 or 2 or 3 described alcohol ether type surfactant polyethylene phthalic monoesters, it is characterized in that described acidic catalyst is the sulfuric acid of phosphorous acid or 98%, its consumption is 0.5～1.5% of a phthalic anhydride weight.
5. according to the preparation method of claim 1 or 2 or 3 described non-alcohol ether type surfactant polyethylene phthalic monoesters, it is characterized in that the described alkali that adds the alkali neutralization is that concentration is that 30% NaOH or concentration are 30% potassium hydroxide.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2006100523866A CN101104139B (en) | 2006-07-10 | 2006-07-10 | Method for preparing alcohol ether type surfactant polyethylene monoester phthalic acid |
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| CN2006100523866A CN101104139B (en) | 2006-07-10 | 2006-07-10 | Method for preparing alcohol ether type surfactant polyethylene monoester phthalic acid |
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| CN101104139A CN101104139A (en) | 2008-01-16 |
| CN101104139B true CN101104139B (en) | 2010-07-28 |
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| CN111138712B (en) * | 2018-11-06 | 2021-12-17 | 杨建强 | Red mud treating agent and preparation method and application thereof |
| CN111825367B (en) * | 2020-06-24 | 2022-01-11 | 中建西部建设建材科学研究院有限公司 | Viscosity reducer for ultra-high performance concrete and preparation method thereof |
| CN114182392A (en) * | 2021-12-17 | 2022-03-15 | 开封大学 | Heat-resistant non-silicon carbon fiber oil agent and preparation and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6172159B1 (en) * | 2000-01-18 | 2001-01-09 | Accures Corporation | Water-reducible polyester resins and urethane coatings produced therefrom |
| CN101085420A (en) * | 2006-06-06 | 2007-12-12 | 杨关雨 | Preparation method of nonionic surfactant polyethylene glycol phthalate |
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- 2006-07-10 CN CN2006100523866A patent/CN101104139B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6172159B1 (en) * | 2000-01-18 | 2001-01-09 | Accures Corporation | Water-reducible polyester resins and urethane coatings produced therefrom |
| CN101085420A (en) * | 2006-06-06 | 2007-12-12 | 杨关雨 | Preparation method of nonionic surfactant polyethylene glycol phthalate |
Non-Patent Citations (4)
| Title |
|---|
| S. N. Tong, et al..聚乙二醇改性不和饱和聚酯树脂.热固性树脂 4.1987,(4),63-66. |
| S. N. Tong, et al..聚乙二醇改性不和饱和聚酯树脂.热固性树脂 4.1987,(4),63-66. * |
| 庞新文等.质谱分析聚醚类非离子表面活性剂.质谱学报7 2.1986,7(2),45-49. |
| 庞新文等.质谱分析聚醚类非离子表面活性剂.质谱学报7 2.1986,7(2),45-49. * |
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